固相萃取-超高效液相色谱-串联质谱法测定菊花中15种吡咯里西啶生物碱毒素  

Determination of 15 kinds of pyrrolizidine alkaloids in Chrysanthemum by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry

作　　者：章豪 杨挺 吴银良 朱勇 ZHANG Hao;YANG Ting;WU Yin-Liang;ZHU Yong(Ningbo Academy of Agricultural Sciences,Laboratory of Quality and Safety Risk Assessment for Agricultural Products(Ningbo),Ministry of Agriculture and Rural Affairs,Ningbo Key Laboratory of Testing and Control for Characteristic Agro-product Quality and Safety,Ningbo 315040,China)

机构地区：[1]宁波市农业科学研究院,农业农村部农产品质量安全风险评估实验室(宁波),宁波市特色农产品质量安全检测与控制重点实验室,宁波315040

出　　处：《食品安全质量检测学报》2024年第21期41-49,共9页Journal of Food Safety and Quality

基　　金：宁波市农业重大专项(2015C110004);宁波市科技惠民项目(2017C50014);宁波市社会发展科技攻关项目(2014C50012);国家农产品质量安全风险评估重大专项(GJFP2020001、GJFP2019019、GJFP201801101、GJFP201701101、GJFP201701104、GJFP201601101、GJFP201501201、GJFP2014011)。

摘　　要：目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定菊花中15种吡咯里西啶生物碱毒素含量的分析方法。方法样品中吡咯里西啶生物碱毒素采用0.1 mol/L硫酸水溶液提取,通过Oasis PRiME MCX固相萃取小柱净化,采用UPLC-MS/MS进行分析。采用Acquity UPLC BEH C18色谱柱分离,以0.1%甲酸水-甲醇溶液为流动相进行梯度洗脱,电喷雾离子源正离子电离,多反应离子监测模式监测,外标法定量。结果15种吡咯里西啶生物碱毒素在一定浓度范围内线性关系良好,相关系数(r2)均大于0.999;定量限为0.50~10.00μg/kg,检出限为0.15~3.00μg/kg;阴性样品的加标回收率为82.8%~92.4%,相对标准偏差为2.1%~4.9%(n=5)。结论该方法准确度和精密度高,耗时短,能同时测定多种菊花样品中的多种吡咯里西啶生物碱毒素含量。Objective To establish a method for determination of 15 kinds of pyrrolizidine alkaloids in Chrysanthemum by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods Pyridolizidine alkaloid toxins in the sample were extracted with 0.1 mol/L sulfuric acid aqueous solution and purified by Oasis PRiME MCX solid phase extraction column,detected by UPLC-MS/MS,separated by the Acquity UPLC BEH C18 column,and using the 0.1%formic acid-methanol solution as the mobile phase for gradient elution,ionized by electrospray ion source positive ion,monitored by multi-reactive ion monitoring mode,quantified by external standard method.Results Good linear relationships were seen for the 15 kinds of pyrrolizidine alkaloids in certain concentration ranges,and the correlation coefficients were more than 0.999.The limits of detection and limits of quantitation for the 15 kinds of pyrrolizidine alkaloids were in the ranges 0.15-3.00 and 0.50-10.00μg/kg,respectively.The recoveries of negative samples ranged from 82.8%to 92.4%,and the relative standard deviations were from 2.1%to 4.9%(n=5).Conclusion The method has high accuracy,high precision and short time consuming,and can simultaneously determine the content of pyrrolizidine alkaloids in a variety of Chrysanthemum samples.

关 键 词：吡咯里西啶生物碱毒素 超高效液相色谱-串联质谱法 Oasis PRiME MCX固相萃取小柱 菊花 

分 类 号：O657.63[理学—分析化学] TS207.5[理学—化学]